摘要
目的 :建立了高效液相色谱法测定血浆中单硝酸异山梨酯浓度。方法 :采用硅胶分析柱 ,以二氯甲烷 -正己烷 -乙腈 -甲醇 (92∶4∶1 5∶2 5 )为流动相 ,卡马西平作内标。样品在碱性条件下用二氯甲烷萃取浓集后进样 ,2 34nm波长下检测 ,按内标法定量。结果 :标准曲线在 2 5～ 16 0 0 μg·L-1范围内有良好线性 ,最低检测浓度为 10 μg·L-1,方法回收率为 96 %～ 10 4% ,日内RSD小于 4 5 % ,日间RSD小于 5 %。结论 :本法具有快速简便 ,灵敏准确等特点 ,已用于单硝酸异山梨酯缓释制剂生物利用度测定 ,结果良好。
Objective:This paper establishes a high performance liquid chromatography for the determination of isosorbide-5-mononitrate(ISMN) in human plasma using carbamazepine as the internal standard.Method:a variable wavelength UV detector and Nuclbosil 5 silica 100A column(250 mm×4 6 mm, 5 μm ) were used. The alkalinized plasma sample was extracted with 3 0 mL methylene chloride . After evaporation of the organic layer, the residue was dissolved in mobile phase and injected onto a column. The mobile phase of methylene chloride-hexane-acetonitrile-methanol(92∶4∶1 5∶2 5) was pumped at 2 0 mL·min -1 through the column. The detector at 0 005 AUFS was set at 234 nm.Results:The retention times for ISMN and carbamazepine were 6 4 min and 7 0 min respectively. Standard curve was linear in the concentration range of 25 to 1 600 μg·L -1 . The detection limit in plasma was 10 μg·L -1 ; and method recovery was 96%～104%; within day RSD less than 4 5%; inter-day RSD less than 5%.Conclusion:This method was found to be simple, rapid, sensitive and accurate for determination of ISMN in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2000年第3期165-167,共3页
Chinese Journal of Pharmaceutical Analysis
